CN104005111B - A kind of Folium Ginkgo cellulose fibre and preparation method thereof - Google Patents
A kind of Folium Ginkgo cellulose fibre and preparation method thereof Download PDFInfo
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- CN104005111B CN104005111B CN201410252665.1A CN201410252665A CN104005111B CN 104005111 B CN104005111 B CN 104005111B CN 201410252665 A CN201410252665 A CN 201410252665A CN 104005111 B CN104005111 B CN 104005111B
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Abstract
The invention discloses a kind of Folium Ginkgo cellulose fibre and preparation method thereof, preparation comprises the following steps: Folium Ginkgo extract is made slow-release microcapsule；Viscose glue is prepared for raw material with cellulose pulp, Folium Ginkgo extract microcapsule emulsion is accounted in dry powder Folium Ginkgo microcapsule therein the ratio of finished fiber weight 1.0～12.0wt%, with blender for place with viscose glue mix homogeneously by the way of injecting before spinning, it is prepared as Folium Ginkgo anti-bacterial fibre cellulose fiber.The Folium Ginkgo anti-bacterial fibre cellulose fiber of the present invention is not only worn slimmer and more graceful, and hygroscopicity, permeability are further enhanced, and production process the most farthest ensure that effective component of ginkgo leaf, it is to avoid waste.The fibre wearability produced is excellent, textile process performance is good, it is antibacterial to resist, health-care effect is more prominent.
Description
Technical field
The present invention relates to modified cellulose technical field, particularly relate to a kind of Folium Ginkgo anti-bacterial fibre cellulose fiber and preparation thereof
Method.
Background technology
China's viscose rayon kind majority is general fibre at present, and functional fiber, fibre in differentiation are little.Though domestic
Know the production technology of color fibre, fire resistance fibre, superfine denier fiber, but the producer forming mass production capabilities is few.
Folium Ginkgo is the dried leaves of Ginkgoaceae plant Ginkgo biloba, autumn leaf the greenest time gather.The extraction extracted from Folium Ginkgo
Thing is exactly a kind of well natural antibacterial agent, is widely used to the fields such as food, medicine, health product, daily-use chemical industry.Folium Ginkgo
Extract is a kind of non-volatile granulated brown solids.Folium Ginkgo is sweet, bitter in the mouth, puckery, flat, returns, lung meridian.Astringe the lung, relieving asthma,
Blood circulation promoting and blood stasis dispelling, the merit of pain relieving.Folium Ginkgo extract primary chemical active component is flavonoid, lactone compound and organic acid thing
Matter etc..Organic acid kind in Folium Ginkgo has a variety of, has summed up fatty acid, hydroxy acid, aminoacid, saccharic acid.Silver
Acid ingredient in Folium Pruni has anti-inflammation, antiviral, antiallergic, anticancer, defying age and effect of anthelmintic parasite killing.In addition its
Can be additionally used in antitumor, speckle dispelling increases face, prevent skin aging etc..
The Folium Ginkgo fiber underwear of bolt is led to as the Chinese patent of Application No. 200910072589.5 discloses a kind of blood pressure lowering,
It is characterized in that this underwear contains Folium Ginkgo fiber, can keep healthy and cure the disease i.e. blood pressure lowering thrombus breaking.
Along with biological extraction and the development of medicine microcapsule technology, the cost of Folium Ginkgo extract is gradually lowered, by Semen Ginkgo
Leaf extract is applied on fiber become possibility.Application No. 00115440.0,00115439.7,00115441.9,
The Chinese patent of 00115444.3 discloses the production method of the polypropylene fibre of a kind of or other function and service, Semen Ginkgo in fiber
Leaf extract medicinal component can discharge under tepid state slowly, and is inhaled by human body by the Repiration of human skin
Receive, make clothing articles or bedding in use have unique health-care effect to human body, and have certain antibacterial merit
Effect.
The most disclosed Folium Ginkgo anti-microbial type fiber broadly falls into the category of synthetic fibers, uses melt-spinning technology to obtain
, on the one hand, synthetic fibers are dependent on greatly petroleum resources, and along with the exhaustion day by day of the energy, exploitation will necessarily be restricted；Another
Aspect, although synthetic fibers strength is prominent, but sucting wet air permeability is poor, wears discomfort, and discomfort is fit to do underclothes dressing, because of
The performance of this antibiotic health care performance is also had a greatly reduced quality.
Because the effective ingredient of Folium Ginkgo extract is essentially Ginkgolides, bilobalide-like and organic acid substance,
Activity is higher, if using traditional cellulose fiber terylene short fiber production technology, as knowledge, pulp is through soda-dip, curing
Adding alkali liquor after carbon yellow and make rayon spinning liquid, use wet spinning spinning process molding after deaeration, maturation, coagulating bath is
Sulphuric acid, the existence of a large amount of acid-alkali salts will certainly cause the loss of most or all biomass extracts, badly influence
The antimicrobial health care function of finished fiber.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, it is provided that a kind of function admirable, textile process performance are good, anti-antibacterial and keep healthy
Cellulose fibre of prominent function and preparation method thereof, solves prior art and causes biomass to run off, short asking action time
Topic.
The technical scheme is that
Folium Ginkgo anti-bacterial fibre cellulose fiber, it is characterised in that: in described fiber, the Folium Ginkgo containing 1.0～12.0wt% carries
Take thing slow-release microcapsule composition.The dry fracture strength of described fiber is 1.70～2.50cN/dtex, wet breaking strength be 0.90～
1.60cN/dtex, dry elongation at break is 16.0～22.0%, and residual sulfur content≤12.0mg/100g, described cellulose fibre is to golden yellow
Staphylococcic bacteriostasis rate >=91.0% of color, to colibacillary suppression ratio >=91.0%, to the suppression ratio of Candida albicans >=
80.0%.
The preparation method of described Folium Ginkgo cellulose fibre, it is characterised in that comprise the following steps:
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 40～55 DEG C, rotating speed
50～60 turns/min, after stirring 60～120min, it is cooled to room temperature, filters after standing 2～3 hours, obtain the silver of 20～25wt%
Folium Pruni extract solution.
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 20～25
Add in reactor, control temperature 80～85 DEG C of heating for dissolving, be subsequently cooled to 50 ± 1 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 0.4～
The emulsifier for mixing mix homogeneously of 1.6%, then high-speed stirred dispersion 20～40min under conditions of 40～45 DEG C, by solution
Inlet temperature 160～180 DEG C, it is spray-dried under the conditions of leaving air temp 70～80 DEG C, obtains particle diameter D90≤1.8 micron, be more than
The microcapsule of particle≤1% of 4 microns.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dissolving tank dispersant, at 38 ± 2 DEG C
Stir 40～60 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 19～24wt%,；
B, in blend tank add stabilizer, weight is ginkgo leaf extract capsule dry powder matter in ginkgo leaf extract capsule
The 0.02～0.1wt% of amount, rotating speed is 50～80 revs/min, and mixing time is deaeration after 30～40 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, by Folium Ginkgo microcapsule by microcapsule powder body therein account for finished fiber weight 1～
The ratio of 12wt%, joins blender by dosing pump, and viscose joins blender by viscose glue effusion meter simultaneously, mixing
It is prepared as Folium Ginkgo microcapsule after Jun Yun and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 80～130g/l, aluminum sulfate 8～12g/l, sodium sulfate 320～350g/l, temperature is
50 ± 2 DEG C, then obtain Folium Ginkgo anti-bacterial fibre cellulose fiber through strand drawing-off and post-processing step.
The preparation method of described Folium Ginkgo anti-bacterial fibre cellulose fiber, it is characterised in that: described stabilizer is dodecyl
The mixed liquor that benzene sulfonic acid sodium salt forms with hexapolyphosphate sodium, ratio is 1: 2.
The preparation method of described Folium Ginkgo anti-bacterial fibre cellulose fiber, it is characterised in that: described emulsifying agent is the soft phosphorus of Semen sojae atricolor
One in fat, sodium lauryl sulphate, tristerin.
The manufacture method of described Folium Ginkgo anti-bacterial fibre cellulose fiber, it is characterised in that: in described spinning process, silk
Bar drawing-off flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off～20～15%,
Drawing-off 20%～40% between dish, plasticizing-bath drawing-off 5%～20%, described post-processing step is cut-out → washing → desulfurization → water
Wash → oil.
The invention has the beneficial effects as follows:
In the case of not affecting normal spinning, Folium Ginkgo extract is made slow-release microcapsule, use injection side before spinning
Formula adds before spinning, and the existence of microcapsule avoids the working substance that the directly contact of Folium Ginkgo extract is caused by strong acid-base
Matter decomposes loss, and in fabric, Folium Ginkgo extract microcapsule discharges effective component of ginkgo leaf slowly along with friction ruptures, and plays
Long-term Anti is antibacterial, the effect of health care, and the Folium Ginkgo fiberoptic fiber that fibre wearability is excellent, textile process performance is good produced
Preparation method.In the Folium Ginkgo cellulose fibre of the present invention, the content of Folium Ginkgo extract effective ingredient runs off less, finished product
Anti-antibacterial, the health care more lasting stability of fiber.Therefore Folium Ginkgo cellulose fibre existing native cellulose fibre
Absorb ventilative, comfortable and easy to wear, discarded after can the advantage of natural degradation, have again anti-antibacterial, that heath-function is strong, effect is lasting is excellent
Point.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.
Embodiment 1 0.78dtex × 32mm Folium Ginkgo anti-bacterial fibre cellulose fiber
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 40 DEG C, rotating speed 50
Turn/min, be cooled to room temperature after stirring 60min, filter after standing 3 hours, obtain the Folium Ginkgo extract solution of 20wt%.
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 20 add
In reactor, control 80 DEG C of heating for dissolving of temperature, be subsequently cooled to 49 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 1.0%
Sodium lauryl sulphate emulsifier for mixing mix homogeneously, then under conditions of 40 DEG C high-speed stirred dispersion 20min, by solution
It is spray-dried under the conditions of inlet temperature 160 DEG C, leaving air temp 70 DEG C, obtains particle diameter D90≤1.8 micron, grain more than 4 microns
The microcapsule of son≤1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dissolving tank dispersant, 38 DEG C of stirrings
50 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 23wt%；
B, in blend tank, add stabilizer dialkyl benzene sulfonic acids sodium and hexapolyphosphate sodium=1: the mixed liquors of 2 compositions, weight
Amount is the 0.05wt% of ginkgo leaf extract capsule dry powder quality in ginkgo leaf extract capsule, and rotating speed is 70 revs/min, stirring
Time is deaeration after 35 minutes；
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight 6wt% by microcapsule powder body therein
Ratio, join blender by dosing pump, viscose joins blender by viscose glue effusion meter simultaneously, after mix homogeneously
It is prepared as Folium Ginkgo microcapsule and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 105g/l, aluminum sulfate 10.5g/l, sodium sulfate 330g/l, temperature is 48 DEG C, strand
Drawing-off flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off～20%, lead between dish
Stretching 20%, plasticizing-bath drawing-off 5%, post-treated step cut-out → washing → desulfurization → wash → oil obtains the antibacterial fibre of Folium Ginkgo
Cellulose fiber.
0.78dtex × 32mm Folium Ginkgo antibacterial cellulose fiber product leading indicator such as the following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Embodiment 2 1.11dtex × 32mm Folium Ginkgo anti-bacterial fibre cellulose fiber
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 48 DEG C, rotating speed 55
Turn/min, be cooled to room temperature after stirring 100min, filter after standing 2 hours, obtain the Folium Ginkgo extract solution of 22.7wt%.
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 25 add
In reactor, control 83 DEG C of heating for dissolving of temperature, be subsequently cooled to 50 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 0.4%
The soft phospholipid emulsifier of Semen sojae atricolor be uniformly mixed, then under conditions of 45 DEG C high-speed stirred dispersion 30min, solution is being entered
Air temperature 180 DEG C, is spray-dried under the conditions of leaving air temp 80 DEG C, obtain particle diameter D90≤1.8 micron, particle more than 4 microns≤
The microcapsule of 1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dispersant of dissolving tank, stir at 40 DEG C
Mix 40 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 24wt%,；
B, in blend tank, add stabilizer dodecylbenzene sodium sulfonate and hexapolyphosphate sodium=1: the mixed liquors of 2 compositions,
Weight is the 0.05wt% of ginkgo leaf extract capsule dry powder quality in ginkgo leaf extract capsule, and rotating speed is 80 revs/min, stirs
The time of mixing is deaeration after 40 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight 1wt% by microcapsule powder body therein
Ratio, join blender by dosing pump, viscose joins blender by viscose glue effusion meter simultaneously, after mix homogeneously
It is prepared as Folium Ginkgo microcapsule and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 96g/l, aluminum sulfate 10g/l, sodium sulfate 342g/l, temperature is 50 DEG C, strand drawing-off
Flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off～10%, drawing-off between dish
30%, plasticizing-bath drawing-off 15%, post-treated step cut-out → washing → desulfurization → wash → oil obtains the antibacterial fibre of Folium Ginkgo
Cellulose fiber.
1.11dtex × 32mm Folium Ginkgo antibacterial cellulose fiber product leading indicator such as the following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Embodiment 3 1.33dtex × 38mm Folium Ginkgo anti-bacterial fibre cellulose fiber
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 55 DEG C, rotating speed 60
Turn/min, be cooled to room temperature after stirring 120min, filter after standing 2.5 hours, obtain the Folium Ginkgo extract solution of 25wt%.
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 25 add
In reactor, control 85 DEG C of heating for dissolving of temperature, be subsequently cooled to 51 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 1.6%
Tristerin emulsifier for mixing mix homogeneously, then under conditions of 45 DEG C high-speed stirred dispersion 40min, solution is existed
Inlet temperature 170 DEG C, is spray-dried under the conditions of leaving air temp 75 DEG C, obtains particle diameter D90≤1.8 micron, particle more than 4 microns
The microcapsule of≤1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dispersant of dissolving tank, stir at 39 DEG C
Mix 42 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 19.9wt%,；
B, in blend tank, add stabilizer dodecylbenzene sodium sulfonate and hexapolyphosphate sodium=1: the mixed liquors of 2 compositions,
Weight is the 0.09wt% of ginkgo leaf extract capsule dry powder quality in ginkgo leaf extract capsule, and rotating speed is 75 revs/min, stirs
The time of mixing is deaeration after 38 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight 12wt% by microcapsule powder body therein
Ratio, join blender by dosing pump, viscose joins blender by viscose glue effusion meter simultaneously, after mix homogeneously
It is prepared as Folium Ginkgo microcapsule and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 112g/l, aluminum sulfate 10.2g/l, sodium sulfate 341g/l, temperature is 51 DEG C, strand
Drawing-off flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off 10%, drawing-off between dish
40%, plasticizing-bath drawing-off 20%, post-treated step cut-out → washing → desulfurization → wash → oil obtains the antibacterial fibre of Folium Ginkgo
Cellulose fiber.
1.33dtex × 38mm Folium Ginkgo antibacterial cellulose fiber product leading indicator such as the following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Embodiment 4 1.67dtex × 38mm Folium Ginkgo antibacterial cellulose fiberoptic fiber
(preparation of (1) ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 53 DEG C, rotating speed 52
Turn/min, be cooled to room temperature after stirring 95min, filter after standing 2 hours, obtain the Folium Ginkgo extract solution of 24.2wt%.
B, the preparation of wall material solution: gelatin mixes with arabic gum in mass ratio 2: 1 and adds at 1: 22.4 in proportion with soft water
Enter in reactor, control 83 DEG C of heating for dissolving of temperature, be subsequently cooled to 49 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 0.8%
Tristerin emulsifier for mixing mix homogeneously, then under conditions of 44 DEG C high-speed stirred dispersion 38min, solution is existed
Inlet temperature 165 DEG C, is spray-dried under the conditions of leaving air temp 72 DEG C, obtains particle diameter D90≤1.8 micron, particle more than 4 microns
The microcapsule of≤1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dispersant of dissolving tank, stir at 36 DEG C
Mix 60 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 19wt%,；
B, in blend tank, add stabilizer dodecylbenzene sodium sulfonate and hexapolyphosphate sodium=1: the mixed liquors of 2 compositions,
Weight is the 0.02wt% of ginkgo leaf extract capsule dry powder quality in ginkgo leaf extract capsule, and rotating speed is 60 revs/min, stirs
The time of mixing is deaeration after 30 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight by microcapsule powder body therein
The ratio of 4.0wt%, joins blender by dosing pump, and viscose joins blender by viscose glue effusion meter simultaneously, mixed
It is prepared as Folium Ginkgo microcapsule after closing uniformly and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 130g/l, aluminum sulfate 12g/l, sodium sulfate 350g/l, temperature is 52 DEG C, and strand leads
Stretching flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off 15%, drawing-off between dish
25%, plasticizing-bath drawing-off 15%, post-treated step cut-out → washing → desulfurization → wash → oil obtains the antibacterial fibre of Folium Ginkgo
Cellulose fiber.
1.67dtex × 38mm Folium Ginkgo antibacterial cellulose fiber product leading indicator such as the following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Embodiment 5 133.3dtex/30F Folium Ginkgo antibacterial cellulose long filament
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 47 DEG C, rotating speed 58
Turning/min, be cooled to room temperature, filter after standing 2.5 hours after stirring 69min, the Folium Ginkgo extract obtaining 21.4wt% is molten
Liquid.
B, the preparation of wall material solution: gelatin mixes with arabic gum in mass ratio 2: 1 and adds at 1: 23.5 in proportion with soft water
Enter in reactor, control 83 DEG C of heating for dissolving of temperature, be subsequently cooled to 50 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 1.1%
The soft phospholipid emulsifier of Semen sojae atricolor be uniformly mixed, then under conditions of 40.8 DEG C high-speed stirred dispersion 26min, solution is existed
Inlet temperature 169 DEG C, is spray-dried under the conditions of leaving air temp 74 DEG C, obtains particle diameter D90≤1.8 micron, particle more than 4 microns
The microcapsule of≤1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dissolving tank dispersant, 38 DEG C of stirrings
40 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 21wt%,；
B, in blend tank, add stabilizer dodecylbenzene sodium sulfonate and hexapolyphosphate sodium=1: the mixed liquors of 2 compositions,
Weight is the 0.1wt% of ginkgo leaf extract capsule dry powder quality in ginkgo leaf extract capsule, and rotating speed is 75 revs/min, stirs
The time of mixing is deaeration after 31 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight 10wt% by microcapsule powder body therein
Ratio, join blender by dosing pump, viscose joins blender by viscose glue effusion meter simultaneously, after mix homogeneously
It is prepared as Folium Ginkgo microcapsule and viscose glue is blended；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 82g/l, aluminum sulfate 8.5g/l, sodium sulfate 320g/l, temperature is 48 DEG C, and strand leads
Stretching flow process is: shower nozzle and drawing-off dish drawing-off → drawing-off dish and solidification rod drawing-off → solidification rod and go sour rod drawing-off；Its process conditions
For: shower nozzle and drawing-off dish drawing-off～4%, drawing-off dish and solidification rod drawing-off 10%, solidify rod and go acid rod drawing-off 1%, described
Post-processing step is washing → desulfurization → salt pickling → oil → be dehydrated → dry → damping → one-tenth cylinder.
The 133.3dtex/30F Folium Ginkgo antibacterial cellulose continuous yarn product leading indicator such as following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Embodiment 6 166.7dtex/30F Folium Ginkgo antibacterial cellulose long filament
(1) preparation of ginkgo biloba extract sustained-release microcapsule:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 51 DEG C, rotating speed 54
Turn/min, be cooled to room temperature after stirring 108min, filter after standing 3 hours, obtain the Folium Ginkgo extract solution of 24wt%.
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 20 add
In reactor, control 804 DEG C of heating for dissolving of temperature, be subsequently cooled to 51 DEG C standby.
C, Folium Ginkgo extract solution is mixed with wall material liquid in mass ratio 1: 2 after, add account for wall material liquid gross weight 1.2%
Sodium lauryl sulphate emulsifier for mixing mix homogeneously, then under conditions of 40 DEG C high-speed stirred dispersion 21min, by molten
Liquid is spray-dried under the conditions of inlet temperature 160 DEG C, leaving air temp 79 DEG C, obtains particle diameter D90≤1.8 micron, more than 4 microns
The microcapsule of particle≤1%.
(2) preparation of cellulose rayon spinning liquid
With cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step prepare viscose glue and spin
Silk liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue:
A, Folium Ginkgo extract microcapsule is joined in the poly-sodium hexametaphosphate solution of dissolving tank dispersant, 36 DEG C of stirrings
40 minutes, in blend tank, after filtration, obtain the ginkgo leaf extract capsule emulsion of 19wt%,；
B, in blend tank add stabilizer, weight is ginkgo leaf extract capsule dry powder matter in ginkgo leaf extract capsule
The 0.02wt% of amount, rotating speed is 50 revs/min, and mixing time is deaeration after 30 minutes.
Prepared by c, blended viscose glue
By spinning front injecting systems, Folium Ginkgo microcapsule is accounted for finished fiber weight 8% by microcapsule powder body therein
Ratio, joins blender by dosing pump, and viscose joins blender by viscose glue effusion meter simultaneously, makes after mix homogeneously
Standby one-tenth Folium Ginkgo microcapsule is blended viscose glue；
(4) spinning and post processing: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning after filtering
Molding, described coagulating bath consist of sulphuric acid 80g/l, aluminum sulfate 8g/l, sodium sulfate 350g/l, temperature is 48 DEG C, strand drawing-off
Flow process is: shower nozzle and drawing-off dish drawing-off → drawing-off dish and solidification rod drawing-off → solidification rod and go sour rod drawing-off；Its process conditions are:
Shower nozzle and drawing-off dish drawing-off 2%, drawing-off dish and solidification rod drawing-off 5%, solidify rod and go acid rod drawing-off 4%, described post processing
Step is washing → desulfurization → salt pickling → oil → be dehydrated → dry → damping → one-tenth cylinder.
The 166.7dtex/30F Folium Ginkgo antibacterial cellulose continuous yarn product leading indicator such as following table prepared:
Note: the antibacterial value in upper table measures according to standard GB/T/T20944.3-2008.
Through the Folium Ginkgo anti-bacterial fibre cellulose fiber prepared by above-described embodiment 1～6 is detected, prepared fiber
The dry fracture strength of cellulose fiber is 1.70～2.50cN/dtex, and wet breaking strength is 0.90～1.60cN/dtex, and dry fracture is stretched
Degree is 16～22%, residual sulfur content≤12.0mg/100g, to bacteriostasis rate >=91.0% of staphylococcus aureus, to escherichia coli
Bacteriostasis rate >=91.0%, suppression ratio >=80.0% to Candida albicans, be satisfied by using requirement.Although it addition, embodiment 1
～the specification of the cellulose fibre prepared by 6 is different, but the analysis found that, the cellulose fluff prepared by embodiment 4
Cellulosic filaments cost prepared by peacekeeping embodiment 6 puts into relatively low, and the cellulose fibre combination property prepared is the highest,
It it is the production and processing method of a kind of optimum.
In the above-described embodiments, the preferred forms of the present invention is described, it is obvious that at the invention structure of the present invention
Under think of, still can make a lot of change.Here, it should be noted that any change made under the inventive concept of the present invention is all incited somebody to action
Fall within the scope of protection of the present invention.
Claims (9)
1. a Folium Ginkgo cellulose fibre, it is characterised in that: in described fiber, the Folium Ginkgo containing 1.0～12.0wt% extracts
Thing microcapsule composition, the preparation method of described Folium Ginkgo extract microcapsule is:
A, Folium Ginkgo extract and soft water in mass ratio 1: 4 being added in dissolution kettle, temperature controls at 40～55 DEG C, rotating speed 50～
60 turns/min, after stirring 60～120min, it is cooled to room temperature, filters after standing 2～3 hours, obtain the Folium Ginkgo of 20～25wt%
Extract solution；
B, the preparation of wall material solution: gelatin mix with arabic gum in mass ratio 2: 1 and with soft water in proportion 1: 20～25 add
In reactor, control temperature 80～85 DEG C of heating for dissolving, be subsequently cooled to 50 ± 1 DEG C standby；
C, Folium Ginkgo extract solution is mixed with wall material solution in mass ratio 1: 2 after, add account for wall material solution gross weight 0.4～
The emulsifier for mixing mix homogeneously of 1.6%, then high-speed stirred dispersion 20～40min under conditions of 40～45 DEG C, by solution
Inlet temperature 160～180 DEG C, it is spray-dried under the conditions of leaving air temp 70～80 DEG C, obtains particle diameter D90 micro-less than or equal to 1.8
Rice, the microcapsule of particle≤1% more than 4 microns.
2. Folium Ginkgo cellulose fibre as claimed in claim 1, it is characterised in that: described emulsifying agent be the soft phospholipid of Semen sojae atricolor, ten
One in sodium dialkyl sulfate, tristerin.
3. the preparation method of a kind of Folium Ginkgo cellulose fibre described in a claim 1, it is characterised in that include following step
Rapid:
(1) preparation of Folium Ginkgo extract microcapsule；
(2) preparation of cellulose rayon spinning liquid；
(3) Folium Ginkgo extract microcapsule is blended the preparation of viscose glue；
(4) spinning and post processing.
4. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 3, it is characterised in that: described cellulose viscose glue
The preparation method of spinning liquid is: with cellulose pulp as raw material, through including impregnating, squeeze, pulverizing, experienced, yellow and dissolving step
Rapid prepared rayon spinning liquid.
5. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 3, it is characterised in that: described Folium Ginkgo extract
Microcapsule is blended the preparation method of viscose glue:
A, being joined by Folium Ginkgo extract microcapsule in the solution of the poly-sodium hexameta phosphate of dispersant of dissolving tank, dispersant adds
Amount is the 0.1～1.0% of Folium Ginkgo extract microcapsule dry powder quality, stirs 40～60 minutes at 38 ± 2 DEG C, is adjusting after filtration
Distribution tank obtains the Folium Ginkgo extract microcapsule emulsion of 19～24wt%；
B, in blend tank add stabilizer, weight is the 0.02～0.1wt% of Folium Ginkgo extract microcapsule dry powder quality, turn
Speed is 50～80 revs/min, and mixing time is deaeration after 30～40 minutes；
Prepared by c, blended viscose glue: by spinning front injecting systems, by Folium Ginkgo extract microcapsule emulsion by microcapsule powder therein
Body accounts for the ratio of finished fiber weight 1～12wt%, joins blender by dosing pump, and rayon spinning liquid passes through viscose glue simultaneously
Effusion meter joins blender, is prepared as Folium Ginkgo microcapsule viscose glue is blended after mix homogeneously.
6. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 3, it is characterised in that: described spinning and post processing
Process is: the Folium Ginkgo microcapsule prepared is blended viscose glue and introduces coagulating bath spinning moulding after filtering, described coagulating bath
Consisting of sulphuric acid 80～130g/L, aluminum sulfate 8～12g/L, sodium sulfate 320～350g/L, temperature is 50 ± 2 DEG C, leads through strand
Stretch and obtain Folium Ginkgo cellulose fibre with post-processing step.
7. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 5, it is characterised in that: described stabilizer is 12
The mixed liquor that sodium alkyl benzene sulfonate forms with hexapolyphosphate sodium, ratio is 1: 2.
8. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 6, it is characterised in that: at described spinning process
In, strand drawing-off flow process is: drawing-off between shower nozzle drawing-off → dish → plasticizing-bath drawing-off；Its process conditions are: shower nozzle drawing-off 20%～
15%, drawing-off 20%～40% between dish, plasticizing-bath drawing-off 5%～20%, described post-processing step for cutting off → washing → de-
Sulfur → wash → oil.
9. the preparation method of Folium Ginkgo cellulose fibre as claimed in claim 6, it is characterised in that: at described spinning process
In, strand drawing-off flow process is: shower nozzle and drawing-off dish drawing-off → drawing-off dish and solidification roller drawing-off → solidification roller and acid removing roller drawing-off；Its
Process conditions are: shower nozzle and drawing-off dish drawing-off 4%～2%, drawing-off dish and solidification roller drawing-off 5%～10%, solidify roller and go acid
Roller drawing-off 1%～4%, described post-processing step be washing → desulfurization → salt pickling → oil → be dehydrated → dry → damping →
Become cylinder.
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| CN106637456A (en) * | 2015-07-24 | 2017-05-10 | 众地家纺有限公司 | Antibacterial, deodorant and efficient deodorizing cellulose fibers and preparation method thereof |
| CN105506766B (en) * | 2016-01-26 | 2017-10-17 | 中科纺织研究院（青岛）有限公司 | A kind of cocos fibre cellulose fiber and preparation method thereof |
| CN105648563B (en) * | 2016-01-27 | 2018-06-05 | 青岛大学 | A kind of cellulose fibre containing aloe extract and preparation method thereof |
| CN108588894A (en) * | 2017-12-29 | 2018-09-28 | 无限极（中国）有限公司 | The preparation method and applications of the mould proof regenerated celulose fibre of antibiosis anti-acarien |
| CN109183171A (en) * | 2018-04-23 | 2019-01-11 | 上海益莎实业有限公司 | A kind of wild Flos Lonicerae viscose rayon preparation method with antibacterial action |
| CN112813516A (en) * | 2020-12-31 | 2021-05-18 | 百事基材料（青岛）股份有限公司 | Viscose macrobiological fiber containing ginkgo, rose, camellia, pomegranate and kudzu root and preparation method thereof |
| CN115074849A (en) * | 2022-07-18 | 2022-09-20 | 湖州草本源新材料有限公司 | Plant cellulose fiber and preparation method thereof |
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